CN114644521A - Preparation method of colored zirconia ceramic powder for false tooth - Google Patents
Preparation method of colored zirconia ceramic powder for false tooth Download PDFInfo
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- CN114644521A CN114644521A CN202210430287.6A CN202210430287A CN114644521A CN 114644521 A CN114644521 A CN 114644521A CN 202210430287 A CN202210430287 A CN 202210430287A CN 114644521 A CN114644521 A CN 114644521A
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- zirconia ceramic
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 239000000843 powder Substances 0.000 title claims abstract description 58
- 239000000919 ceramic Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 26
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 25
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012700 ceramic precursor Substances 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 17
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 6
- BSWXAWQTMPECAK-UHFFFAOYSA-N 6,6-diethyloctyl dihydrogen phosphate Chemical compound CCC(CC)(CC)CCCCCOP(O)(O)=O BSWXAWQTMPECAK-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- 229920000609 methyl cellulose Polymers 0.000 claims description 4
- 239000001923 methylcellulose Substances 0.000 claims description 4
- 235000010981 methylcellulose Nutrition 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims description 4
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229910003447 praseodymium oxide Inorganic materials 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000003232 water-soluble binding agent Substances 0.000 claims description 4
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000230 xanthan gum Substances 0.000 claims description 2
- 229920001285 xanthan gum Polymers 0.000 claims description 2
- 235000010493 xanthan gum Nutrition 0.000 claims description 2
- 229940082509 xanthan gum Drugs 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000004040 coloring Methods 0.000 abstract description 15
- 229910000314 transition metal oxide Inorganic materials 0.000 abstract description 8
- 239000007787 solid Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000049 pigment Substances 0.000 abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 6
- -1 rare earth metal ions Chemical class 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 230000002411 adverse Effects 0.000 abstract description 3
- 238000000280 densification Methods 0.000 abstract description 3
- 239000006104 solid solution Substances 0.000 abstract description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 13
- 238000005303 weighing Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000000462 isostatic pressing Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000001055 chewing effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 150000003746 yttrium Chemical class 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
- A61C13/08—Artificial teeth; Making same
- A61C13/083—Porcelain or ceramic teeth
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9661—Colour
Abstract
The invention relates to a preparation method of colored zirconia ceramic powder for false teeth, which comprises the following steps: preparing zirconium oxychloride into an aqueous solution, and adding a metal oxide and yttrium oxide to dissolve to obtain a solution; then carrying out hydrothermal reaction; adjusting the pH of the solution after the hydrothermal reaction to be alkaline to obtain slurry; washing the slurry with water until the conductivity is below 2500 mu s/cm; and drying the slurry after washing, adding a dispersant, grinding, sieving, calcining to obtain a colored zirconia ceramic precursor, adding a binder into the colored zirconia ceramic precursor, and performing ball milling to obtain the colored zirconia ceramic powder. Solid metal oxide is directly dissolved in zirconium oxide in a solid solution mode, and after rare earth metal ions are colored, the use amount of other transition metal oxide pigments is reduced, so that the influence of the transition metal oxide pigments enriched in a grain boundary on sintering densification is reduced, the adverse effect on the strength of the material is avoided, and the coloring is more stable and uniform.
Description
Technical Field
The invention relates to a preparation method of colored zirconia ceramic powder for false teeth, belonging to the technical field of ceramic materials.
Background
The artificial tooth refers to a false tooth which is inserted for recovering the functions of chewing, beauty, pronunciation and the like after the tooth is fallen off or pulled out. The raw material commonly used for manufacturing the false tooth is zirconia ceramics, the false tooth often needs to meet certain color conditions due to aesthetic requirements, colored zirconia ceramic powder meets the individual requirements of modern society, and the colored zirconia ceramics have wide market prospect, and are usually prepared by the following methods:
one is to partially sinter the white zirconia to 50-60% theoretical density, then soak it in a salt solution containing one or more transition metals and rare earth oxides to dye it, then dry it and sinter it further. Coloured solution, porous zirconia article as described in patent CN 104918900A. The main disadvantages of this type of impregnation are: the coloring agent is difficult to be uniformly dispersed in the ceramic matrix, the repeatability is poor, the coloring uniformity of the zirconia powder depends on the technique of an operator, the sensory quality of the product is easily low, and the yield is low. In addition, the coloring solution generally contains first transition metal elements, such as Fe, Mn and the like, which easily causes uneven coloring; the first transition metal element can only exist in the product boundary in general; the presence of coloring ions in the grain boundaries may reduce the light transmittance of the dental zirconia product, and if the content of coloring ions in the grain boundaries is high, the strength of the dental zirconia product may be reduced. In addition, in order to prevent coloring ions from precipitating out of the solution and to improve the stability of the coloring solution, it is necessary to add a complexing agent or increase the acidity of the coloring solution. The method has high requirements on the quality of the zirconia blank, and the dyeing solution is difficult to penetrate into the blank, so that the drying operation of the blank is increased, the process is complex, and the final product has a light colored layer and poor repeatability.
Secondly, preparing colored zirconia powder by taking soluble rare earth salts as a coloring agent, soluble yttrium salts as a stabilizing agent and zirconium oxychloride as a matrix of matrix zirconia by adopting a coprecipitation method, and then molding by adopting a dry pressing, direct isostatic pressing and isostatic pressing combination mode; and placing the molded blank into a sintering furnace for presintering to obtain the dental colored zirconia blank. For example, CN 101926732a provides a method for preparing dental colored nano zirconia. In the method, the transition metal ions can only be distributed at the grain boundary in the ceramic matrix, the melting point of the transition metal oxide is low, and the transition metal oxide is easy to melt in the sintering preparation process, so that the enrichment and segregation of components on the grain boundary are caused, and the color development and the mechanical strength of the product are influenced. Although the rare earth metal ions can be dissolved into the zirconia lattice in a solid solution, when the rare earth metal ions enter the tetragonal zirconia lattice which is already partially stabilized by yttrium, the stability of the tetragonal zirconia is improved, and the phase transformation toughening effect is influenced.
Chinese patents CN1566021 and CN102659401A also report methods for preparing black and gray zirconia ceramics under graphite reducing atmosphere, but similar coloring methods need to be performed under reducing or vacuum conditions.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of colored zirconia ceramic powder for false teeth, wherein non-ferrous metal ions are dissolved in zirconia crystal lattices in a solid way, and do not influence the stability of tetragonal zirconia; solid metal oxide is directly dissolved in zirconium oxide in a solid solution mode, and after rare earth metal ions are colored, the use amount of other transition metal oxide pigments is reduced, so that the influence of the transition metal oxide pigments enriched in a grain boundary on sintering densification is reduced, the adverse effect on the strength of the material is avoided, and the coloring is more stable and uniform.
The technical scheme for solving the technical problems is as follows: a preparation method of colored zirconia ceramic powder for false teeth comprises the following steps:
s1, preparing zirconium oxychloride into an aqueous solution, and adding metal oxide and yttrium oxide to dissolve the aqueous solution to obtain a solution;
s2, carrying out hydrothermal reaction on the solution obtained in the S1;
s3, adjusting the pH of the solution after the hydrothermal reaction to be alkaline to obtain slurry;
s4, washing the slurry of S3 with water until the conductivity is below 2500 mu S/cm;
s5, drying the slurry washed by the water of the S4, adding a dispersing agent, grinding, sieving and calcining to obtain a colored zirconia ceramic precursor;
and S6, adding a binder into the colored zirconia ceramic precursor obtained in the step S5, and performing ball milling to obtain the colored zirconia ceramic powder.
Further, the colored zirconia ceramic powder comprises the following raw materials in parts by weight: 94.1-97.6 parts of zirconium oxychloride; 0.07-0.18 part of metal oxide; 1.9-3.2 parts of yttrium oxide; 0.3-2.0 parts of a dispersing agent; 0-0.5 part of binder.
Preferably, the raw materials of the colored zirconia ceramic powder comprise, by weight: 94.1 parts of zirconium oxychloride; 0.9 part of metal oxide; 1.9 parts of yttrium oxide; 1.8 parts of a dispersing agent; 1.3 parts of a binder.
Further, the metal oxide is one or a combination of erbium oxide, praseodymium oxide and iron oxide.
Further, the dispersing agent is one or more of absolute ethyl alcohol, polyacrylamide, triethyl hexyl phosphoric acid or stearic acid.
Further, the binder is a water-soluble binder, and the water-soluble binder is one or more of polyvinyl alcohol, xanthan gum, polyethylene oxide, methyl cellulose or polyvinylpyrrolidone.
Further, in S1, zirconium oxychloride is prepared into 0-2 mol/L aqueous solution, then metal oxide and yttrium oxide are added, and the solution is heated to 50-65 ℃ for dissolution.
Further, in S2, the temperature condition of the hydrothermal reaction is 120-200 ℃, and the hydrothermal reaction time is 1-96 hours.
Further, in S3, adjusting the pH of the solution after the hydrothermal reaction to 8-14 by using 10-25% by mass of ammonia water.
Further, in S4, the centrifugal speed in the water washing process is 4000-12000 rpm.
Further, the slurry washed with water in S5 is dried at 95 ℃ to realize drying, and the temperature of the calcining process is 900-1100 ℃. The calcination temperature indirectly affects the strength of the product.
Further, in S6, the ball milling is wet ball milling, the rotation speed of the ball mill is 300-800 rpm, and the ball milling time is 1-2 hours; the grain diameter of the colored zirconia ceramic powder after ball milling treatment is 0.1-2 μm. The ball mill is a planetary ball mill, but is not limited thereto.
The invention has the beneficial effects that:
1) the false tooth made of the color zirconia ceramic powder for the false tooth obtained by the invention has higher hardness, and solves the problems of frangibility, low glossiness, poor color development and low transparency of the all-ceramic material;
2) the invention dissolves the non-ferrous metal ion in the zirconia, wherein after the rare earth metal ion is colored, the consumption of other transition metal oxide pigments is reduced, thereby reducing the influence of the transition metal oxide pigments enriched in the grain boundary on sintering densification and avoiding the adverse effect on the material strength;
3) the zirconia ceramic powder prepared by the method is uniform in coloring, high in glossiness and transparency, meets the individual requirements of the modern society, and has wide market prospect;
4) the method for manufacturing the colored zirconia ceramic powder for the false tooth has the advantages of simple and convenient materials, simple and standard operation, further perfection of process parameters, improvement of the utilization rate of finished products and reduction of the production cost.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
A preparation method of colored zirconia ceramic powder for false teeth comprises the following steps:
s1, weighing: weighing the following raw materials in parts by weight for later use:
zirconium oxychloride: 96.3 parts of; metal oxide(s): 0.09 part; yttrium oxide: 1.9 parts; absolute ethanol: 1.2 parts; methyl cellulose: 0.5 part. Wherein the metal oxide is erbium oxide.
S2, preparing a colored zirconia ceramic precursor, which comprises the following steps:
s21, dissolving: and (3) preparing 1.2mol/L aqueous solution from the zirconium oxychloride weighed in the S1, adding the weighed metal oxide and yttrium oxide solid, and heating to 50-65 ℃ for dissolving.
S22, hydrothermal: and (3) placing the solution dissolved in the S21 into a reaction kettle, and carrying out hydrothermal reaction at the hydrothermal temperature of 130 ℃ for 20 hours.
S23, regulating the PH value: and (3) adjusting the hydrothermal solution of S22 to pH 10 by using 25 mass percent ammonia water.
S24, washing: and washing the slurry neutralized by S23 with pure water until the conductivity reaches below 1500 mu S/cm, wherein the centrifugal speed during washing is 6000 rpm.
S25, drying: and drying the slurry washed by the water of S24 at 95 ℃, adding absolute ethyl alcohol, grinding and sieving by a 60-mesh sieve.
S26, calcining: and placing the dried powder of S25 in a crucible, and calcining for 1.5h at 990 ℃ to obtain the colored zirconia ceramic precursor.
S3, ball milling: adding methyl cellulose, and placing the colored zirconia ceramic precursor calcined by S26 in a planetary ball mill for ball milling for 2h at the rotating speed of 500rpm to obtain colored zirconia ceramic powder. The grain size of the colored zirconia ceramic powder is 0.2 um.
Example 2
A preparation method of colored zirconia ceramic powder for false teeth comprises the following steps:
s1, weighing: weighing the following raw materials in parts by weight for later use:
zirconium oxychloride: 97.6 parts; metal oxide(s): 0.07 part; yttrium oxide: 1.9 parts; triethylhexylphosphoric acid: 0.33 part; polyvinylpyrrolidone: 0.1 part. Wherein the metal oxide is praseodymium oxide.
S2, preparing a colored zirconia ceramic precursor, which comprises the following steps:
s21, dissolving: and (3) preparing 1.5mol/L aqueous solution from the zirconium oxychloride weighed in the S1, adding the weighed metal oxide and yttrium oxide solid, and heating to 50-65 ℃ for dissolving.
S22, hydrothermal: and (3) placing the solution dissolved in the S21 into a reaction kettle, and carrying out hydrothermal reaction at the hydrothermal temperature of 120 ℃ for 16 h.
S23, regulating the PH value: the hydrothermal solution of S22 was adjusted to pH 8 with 20% by mass aqueous ammonia.
S24, washing: the slurry neutralized by S23 was washed with pure water until the conductivity reached 2000. mu.s/cm or less, and the centrifugation speed during the washing was 8000 rpm.
S25, drying: and drying the slurry obtained by washing the S24 at 95 ℃, adding triethylhexyl phosphoric acid, grinding and sieving by a 60-mesh sieve.
S26, calcining: and placing the dried powder of S25 in a crucible, and calcining at 1100 ℃ for 1.0h to obtain the colored zirconia ceramic precursor.
S3, ball milling: and adding polyvinylpyrrolidone, and placing the calcined colored zirconia ceramic precursor of S26 in a planetary ball mill for ball milling for 1h at the rotating speed of 800rpm to obtain colored zirconia ceramic powder. The grain size of the colored zirconia ceramic powder is 0.35 um.
Example 3
A preparation method of colored zirconia ceramic powder for false teeth comprises the following steps:
s1, weighing: weighing the following raw materials in parts by weight for later use:
zirconium oxychloride: 95.97 parts of a binder; metal oxide(s): 0.13 part; yttrium oxide: 2.1 parts; stearic acid: 1.5 parts; polyethylene oxide: 0.3 part. Wherein the metal oxide is iron oxide.
S2, preparing a colored zirconia ceramic precursor, which comprises the following steps:
s21, dissolving: and (3) preparing 1.0mol/L aqueous solution from the zirconium oxychloride weighed in the S1, adding the weighed metal oxide and yttrium oxide solid, and heating to 50-65 ℃ for dissolving.
S22, hydrothermal: and (3) placing the solution dissolved in the S21 into a reaction kettle, and carrying out hydrothermal reaction at the hydrothermal temperature of 160 ℃ for 24 hours.
S23, regulating the PH value: the hydrothermal solution of S22 was adjusted to pH 9.5 with 15% by mass aqueous ammonia.
S24, washing: the slurry neutralized in S23 was washed with pure water until the conductivity became 1000. mu.s/cm or less, and the centrifugal speed during the washing was 9000 rpm.
S25, drying: and (3) drying the slurry washed by the water of S24 at 95 ℃, adding stearic acid, grinding and sieving by a 60-mesh sieve.
S26, calcining: and placing the dried powder of S25 in a crucible, and calcining for 1.5h at 1000 ℃ to obtain the colored zirconia ceramic precursor.
S3, ball milling: adding polyethylene oxide, and placing the colored zirconia ceramic precursor calcined by S26 into a planetary ball mill for ball milling at the rotating speed of 500rpm for 1.5h to obtain colored zirconia ceramic powder. The grain size of the colored zirconia ceramic powder is 0.15 um.
Example 4
A preparation method of colored zirconia ceramic powder for false teeth comprises the following steps:
s1, weighing: weighing the following raw materials in parts by weight for later use:
zirconium oxychloride: 94.1 parts of; metal oxide(s): 0.9 part; yttrium oxide: 1.9 parts; polyacrylamide: 1.8 parts; polyvinyl alcohol: 1.3 parts. Wherein the metal oxide is praseodymium oxide.
S2, preparing a colored zirconia ceramic precursor, which comprises the following steps:
s21, dissolving: and (3) preparing the zirconium oxychloride weighed in the S1 into 0.7mol/L aqueous solution, adding the weighed metal oxide and yttrium oxide solid, and heating to 50-65 ℃ for dissolving.
S22, hydrothermal: and (3) placing the solution dissolved in the S21 into a reaction kettle, and carrying out hydrothermal reaction at the hydrothermal temperature of 140 ℃ for 18 h.
S23, regulating the PH value: and adjusting the pH of the hydrothermal solution of S22 to 9.1 by using 10 mass percent ammonia water.
S24, washing: the slurry neutralized in S23 was washed with pure water until the conductivity became 100. mu.s/cm or less, and the centrifugation speed during washing was 12000 rpm.
S25, drying: and (3) drying the slurry washed by the water of S24 at 95 ℃, adding polyacrylamide, grinding and sieving by a 60-mesh sieve.
S26, calcining: and placing the dried powder of S25 in a crucible, and calcining for 5 hours at 900 ℃ to obtain the colored zirconia ceramic precursor.
S3, ball milling: adding polyvinyl alcohol, and placing the calcined colored zirconia ceramic precursor of S26 into a planetary ball mill for ball milling at the rotation speed of 300rpm for 2 hours to obtain colored zirconia ceramic powder, wherein the particle size of the obtained colored zirconia ceramic powder is 0.1 um.
Comparative example 1
The same procedure as in example 4 was carried out for the preparation of colored zirconia ceramic powder for dental prostheses, except that the PH was adjusted to 7 in the step of S23, to finally obtain a colored zirconia ceramic powder having a particle size of 0.25 um.
Comparative example 2
The same procedure as in example 4 was carried out for the preparation of colored zirconia ceramic powder for dental prostheses, except that the water washing process of S24 was not carried out, and the grain size of the resultant colored zirconia ceramic powder was 0.5 um.
Comparative example 3
The same procedure as in example 4 was carried out for the preparation of colored zirconia ceramic powder for dental prosthesis, except that the temperature in the calcination process of S26 was 1150 deg.C, and the particle size of the resultant colored zirconia ceramic powder was 0.6 um.
Comparative example 4
The same procedure as in example 4 was carried out for the preparation of colored zirconia ceramic powder for dental prosthesis, except that the temperature in the calcination process of S26 was 850 deg.C, and the particle size of the resultant colored zirconia ceramic powder was 0.4. mu.m.
Comparative example 5
The same procedure as in example 4 was carried out for the preparation of colored zirconia ceramic powder for dentures, except that no yttria was added, and the particle diameter of the finally obtained colored zirconia ceramic powder was 0.6 um.
The products of examples 1-4 and comparative examples 1-5 were tested for performance using conventional assay methods and the results are given in the following table:
as can be seen from the performance test data of examples 1-4 and comparative examples 1-4, the washing conductivity, pH and calcination temperature all affect the strength and coloring of the product. The removal of impurities can be influenced by the excessively high washing conductivity, so that the color and the breaking strength of the product are influenced; too high pH can cause environmental pollution and waste resources, while too low pH can affect the conversion rate of yttrium oxide, thereby affecting the stability of the product; the density and strength of the product are indirectly affected by the calcining temperature which is too high or too low. In addition, the colored zirconia ceramic powder with good coloring effect and high strength can be obtained by combining the yttria, the zirconium oxychloride and the metal oxide. This can be said: the method can effectively obtain products with high strength and good coloring effect, and is more beneficial to application in false teeth.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of colored zirconia ceramic powder for false teeth is characterized by comprising the following steps:
s1, preparing zirconium oxychloride into an aqueous solution, and adding metal oxide and yttrium oxide to dissolve the aqueous solution to obtain a solution;
s2, carrying out hydrothermal reaction on the solution obtained in the S1;
s3, adjusting the pH of the solution after the hydrothermal reaction to be alkaline to obtain slurry;
s4, washing the slurry of S3 with water until the conductivity is below 2500 mu S/cm;
s5, drying the slurry washed by the water of the S4, adding a dispersant, grinding, sieving and calcining to obtain a colored zirconia ceramic precursor;
and S6, adding a binder into the colored zirconia ceramic precursor obtained in the step S5, and performing ball milling to obtain the colored zirconia ceramic powder.
2. The method for preparing a colored zirconia ceramic powder for a denture according to claim 1, wherein the colored zirconia ceramic powder comprises the following raw materials in parts by weight: 94.1-97.6 parts of zirconium oxychloride; 0.07-0.18 parts of metal oxide; 1.9-3.2 parts of yttrium oxide; 0.3-2.0 parts of a dispersing agent; 0-0.5 part of binder.
3. The method for preparing a colored zirconia ceramic powder for a denture according to claim 1, wherein the colored zirconia ceramic powder comprises the following raw materials in parts by weight: 94.1 parts of zirconium oxychloride; 0.9 part of metal oxide; 1.9 parts of yttrium oxide; 1.8 parts of a dispersing agent; 1.3 parts of a binder.
4. The method for preparing a colored zirconia ceramic powder for a denture according to claim 1, wherein the metal oxide is one or a combination of erbium oxide, praseodymium oxide and iron oxide.
5. The method for preparing a colored zirconia ceramic powder for dental prosthesis according to claim 1, wherein the dispersant is one or more of absolute ethyl alcohol, polyacrylamide, triethylhexylphosphoric acid or stearic acid.
6. The method for preparing a colored zirconia ceramic powder for a denture as claimed in claim 1, wherein the binder is water soluble binder, the water soluble binder is one or more of polyvinyl alcohol, xanthan gum, polyethylene oxide, methyl cellulose or polyvinylpyrrolidone.
7. The method for preparing a colored zirconia ceramic powder for a denture as claimed in claim 1, wherein in S1, the zirconium oxychloride is prepared into 0-2 mol/L aqueous solution, then the metal oxide and the yttria are added, and the mixture is heated to 50-65 ℃ for dissolution.
8. The method for preparing the colored zirconia ceramic powder for the denture as claimed in claim 1, wherein in S2, the temperature of the hydrothermal reaction is 120-200 ℃ and the hydrothermal reaction time is 1-96 h.
9. The method for preparing the colored zirconia ceramic powder for the denture according to claim 1, wherein in S3, the solution after the hydrothermal reaction is adjusted to pH 8-14 by ammonia water with the mass fraction of 10% -25%.
10. The method for preparing the colored zirconia ceramic powder for the denture as claimed in claim 1, wherein in S6, the ball milling is wet ball milling, the rotation speed of the ball mill is 300-800 rpm, and the ball milling time is 1-2 h; the grain diameter of the colored zirconia ceramic powder after ball milling treatment is 0.1-2 μm.
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